Journal of the Balkan Tribological Association

Vol. 24, No 2, 250–262 (2018)

Lubrication – metalworking fluids.

DEVELOPMENT OF METALWORKING FLUIDS FOR PROCESSING

AND SHIPMENT OF FABRICATED METAL PRODUCTS

YE. J. AGHAZADA*, V. M. ABBASOV, S. E. ABDULLAYEV,

EL. K. HASANOV, UL. J. YOLCHUYEVA

‘Acad. Yu.G. Mamedaliyev’Institute of Petrochemical Processes, Azerbaijan

National Academy of Sciences, 30 Khojali ave., AZ1025 Baku, Azerbaijan
E-mail: yaghazada@yahoo.com

ABSTRACT

As the technology is developing rapidly, corrosion protection of the metal appli-

ances is one of the most actual problems for both global and local industries of
modern world. The purpose of the work is to synthesize multifunctional highly
adhesive nitrogen containing corrosion inhibitors with different molecular mass-
es on the basis of local feedstocks with enough reserves and to prepare high –
performance metalworking fluids by using them as additives. The metalworking
fluids (MWF) and lubricants have been prepared from liquid rubber and different
inhibitors in T-30 turbine oil medium. The experiments have been done on the
steel plates in condensation and environment phases in the experiment chamber.
The physical and chemical properties of the produced compositions have been
studied, and the morphology of inhibited carbon steel surface was analyzed and
characterized by using Fourier transformer infrared (FTIR) and scanning elec-
tron microscopy (SEM) techniques. Effect of temperature on inhibition efficien-
cy, adhesion and thermodynamic parameters have also been reported. Thermal
analyzer was used for the thermogravimetric analysis (TG/DTA) of the prepared
MWF. As a result of the experiments, it was revealed that when the synthesized
amidoamines and nitro-compounds are highly adhesive to steel, and applied as
MWF and lubricants in the form of composition, the protection effect of metal
plates is higher.
The results show that the metalworking fluids and lubricants can be industri-
ally applied as an effective protection for processing and shipment of metal based
products.
Keywords: corrosion, inhibitor, amidoamine, liquid rubber, nitro compound.

* For correspondence.

250
AIMS AND BACKGROUND

As the technology is developing rapidly, corrosion protection of the metal appli-

ances is one of the most actual problems for both global and local industries of
modern world. Regardless of their operational conditions, metal constructions
show thermodynamically unstable state as they react with the aggressive part of
the environment and corrode. In aggressive medium, the use of organic corrosion
inhibitors is one of the most common, effective and economical methods to pro-
tect metals1–3. Organic compounds containing functional electronegative groups
and electrons in triple and conjugated double bonds have become widely accepted
as effective corrosion inhibitors in various media. The inhibitory effect of an
organic inhibitor is reinforced by the presence of hetero adsorption active centre
such as sulphur (S), nitrogen (N) and oxygen (O) atoms in its molecule. In addi-
tion to the molecular electronic structure with a number of these active centers,
the molecular size, the mode of adsorption, the formation of metallic complexes,
and the projected area of the inhibitor on the metallic surface also influence the
efficiency of inhibition4–7. Former studies concluded that the adsorption on the
mild steel surface depends mainly on the physicochemical properties of the inhib-
itor group such as the planarity of the system, the presence of multiple adsorption
active centres with alone pair and or π orbitals, the electronic density of the donor
atom and the molecular size. Therefore, the choice of effective inhibitors is based
on their structure, mechanism of action and electron donating ability8–10.
The purpose of the work is to synthesize multifunctional nitrogen containing
corrosion inhibitors with different molecular masses on the basis of local feed-
stocks with enough reserves and to prepare high – performance metalworking
fluids by using them as additives4,7,11,12. The widespread investigation of the in-
hibitors in the MWF is based on its economic efficiency and simple structure of
application technology. The addition of a small amount of an inhibiting substance
to the aggressive system is enough for protecting the metal without any changes
to the current technical system13–16.
Lubricants are used in order to protect metal based appliances and equip-
ment during the storage and transportation time.
In this proceeding, the compositions of the T-30 turbine oil with liquid rub-
ber, the complex of polyethylene polyamine with natural petroleum acid and ni-
trocompounds, which are synthesized on the basis of C14H28 α-olefins have been
investigated at different ratio and in various contents as MWF.

EXPERIMENTAL

The 1st type of the reagent, which is tested as an inhibitor in the MWF is the
complex of amidoamines with nitro compound. The mole ratios of the NPA and
251
DETA, TETA and PEPA are different in amidoamine synthesis (T = 130 – 140°C).
It should be mentioned that it is possible to synthesize amidoamines, which con-
tain a number of amine group in the molecule by changing the mole ratio of the
acid and amine.
The NPA, which is used in the process, has been obtained by the dearomatiza-
tion of the diesel fraction with the boiling range of 220–350°C. The dearomatization
process has been operated with the extraction method. N-methyl pyrrolidone has
been used as an extract. The physical and chemical properties of the fraction, which
was obtained from the extraction process were studied and given in Table 1.

Table 1. The physical and chemical properties of the fraction NPA

Kinematic Total
Density Molecular Freezing Boiling Aromatic
Refraction viscosity sulfur
ρ420 weight tempera- tempera- hydrocarbos
nd20 at 20°C content
(g/cm3) Mr (g/mol) ture (°C) ture (°C) (% by mass)
(mm2/s) (%)
0.8294 1.4677 187 –51 220–340 ~5.52 ~ 0.03 ~1

The composition of the solution, which contains synthesized amidoamine

and nitro compound with the polybutadiene based liquid rubber has been pre-
pared and tested on steel plates. The liquid rubber, which is used in the process
has been synthesized on the basis of stereo regular structured 1,4 cis – polybutadi-
ene (low molecular weight, Mr ~1800-3000), which has a wide range of industrial
application microstructure: 1,4 cis-75~80% ; 1,4 trans-18~22% ; 1,2-units-2~7%,
number of units~80). The cis- position of the methyl groups in liquid rubber facil-
itates the adsorption on the metal surface16,17. Nitro compound is synthesized by
using treating C14H28, which is produced by the oligomerization of ethylene with
nitro compound with nitric acid in optimal condition (sodium nitrite is used as an
inisiator). T-30 turbine oil has been used as a solvent. The amount of the active
components was 1:1:1 (in grams). The production process of lubricants based on
conservation liquids having different concentrations has been conducted by add-
ing 10 % (by mass) of technical paraffin to the selected liquids.
The physical and chemical properties (Table 2) of the composition of inhib-
itor have been investigated and its content has been proved by IR spectrosopy
method18–21.

Table 2. Main physical properties of conservation fluids

Name of the Samples

Name of the property ASTM
device I II III IV V
Freezing point ˚C Stanhope Seta ASTM D2386 –25 –28 –30 –30 –30
Viscosity mm2/s, ˚C 40 TW4000 ASTM D445 53.99 65.59 56.47 62.05 65.3
Viscosity, mm2/s, ˚C 100 TW4000 ASTM D445 7.63 8.64 7.98 8.32 8.51
Density, g/cm3 DMA 4500 M D5002 0.9090 0.9058 0.9093 0.9015 0.9042

252
Code number and structure of the samples
I – Amidoamine (NPA+PEPA 2:1)
R - C - HN - CH2 - CH2 (NH - CH2 - CH2)4 - NH CH2 - CH2 - NH - C - R
=

=
O O

II – Amidoamine (NPA+DETA2:1)
R - C - NH - CH2 - CH2 - NH - CH2 - CH2 - NH - C - R
=

=
O O

III – Amidoamine (NPA+TETA 3:1)

R - C - NH - CH2 - CH2 - N - CH2 - CH2 - NH - CH2 - CH2 - NH - C - R

=
=

=
C O
O O
R
IV – Amidoamine (NPA+TETA 2:1)
R - C - NH - CH2 - CH2 - NH - CH2 - CH2 - NH - CH2 - CH2 - NH - C - R
=

=
O O

V – Amidoamine (NPA+PEPA 3:1)

R - C - HN - CH2 - CH2 - N - CH2 - CH2 (NH - CH2 - CH2)3 - NH - CH2 - CH2 - NH
=

O C = O C = O
R R

In order to determine the identity of the conservation liquid, 5 different points

have been chosen on a given sample and IR spectra have been evaluated. The
content of the composition has been tested by IR- Fourier LUMOS (BRUKER)
microscope in the range of 600–4000 cm–1 wavelength.
The following wavelength has been obtained by the spectral analysis of the
MWF of the inhibitor (Sample I), which shows the maximal efficiency.
The valence and deformation oscillations of CH3 and CH2 groups have
been observed in the wavelength of 721, 1380, 1470, 2827, 2873, 2939 cm–1 and
2967  cm–1 in the IR spectra of the 1st point. At the same time, the deformation
oscillations of C – H bond of CH2 naphthenic group are observed in the wave-
length of 966 cm–1. The valence oscillations of C – NO2 group are observed in
the wavelength of 1531 cm–1 and 1558 cm–1 and the C = O group, which belongs
to amidoamines, shows valence oscillations in the wavelength of 1708 cm–1. The
comparison of the IR spectrum of all 5 points on the sample shows that they are
253
Fig. 1.1. The microscopic view of 5 selected
points in sample
Fig. 1.2. IR spectra of the 1st point

Fig. 1.3. IR spectra of the 2nd point Fig. 1.4. IR spectra of the 3rd point

Fig. 1.5. IR spectra of the 4th point Fig. 1.6. IR spectra of the 5th point

practically the same, which proves that the MWF are distributed on the metal
surface homogeneously.
STA-449 F3, NETZSCH thermal analyser was used for the thermogravimet-
ric analysis (TG/DTA – change in mass depending on the temperature and differ-
254
ential thermal analysis) of the prepared MWF (Fig. 2). The processes have been
operated by using nitrogen gas flow and by increasing the temperature by 20°C
per minute. The evaluation of thermal analysis of the Sample I shows that there is
no chemical change in the STA (Simultaneous Thermal Analysis) curve, the peak
at 360°С coincides with the complete disintegration of the composition22,23. The
component that has less thermal stability in the studied MWF is nitro compound.
Hence, nitro compounds are decomposed at temperatures above 600°C, then ami-
do amines and liquid rubber are decomposed respectively. The dependence of the
change in the mass loss on the temperature is given in the Table 3.
Because of the uniform distribution of the components in the T-30 oil me-
dium and thermostability property of amidoamines, metalworking fluids can be
utilized for a long time without losing their quality.
The specific contact method has been used in order to determine the resistivi-
ty (specific conductance) of the compositions. The measurement process has been
operated by the E6-13A teraohmmeter. The measurement places are cleaned with
alcohol before each process and the distance between electrodes is determined.
Then, the substance is poured until the area between electrodes is filled and the
resistivity is measured. The resistivity is calculated according to r = pr2/d equa-
tion and the conductance is determined by the following equation: σ = 1/r. The
physical components in the formulae are following: r – resistance, p – constant,
σ – conductance, r – radius of the measurement electrode, d – distance between
electrodes24,25. The determined electrical conductivity values of the samples are
shown in the Table 4.

Fig. 2. TG/DTA curves of the Sample 1

255
 Table 3. Changes due experiment with temperature

256
Electrıcal Electrıcal Electrıcal
Tempera- Special Special resis- Special
conductiv- conductiv- conductiv- Tempera- Mass loss Mass
No ture resistance No tance No resistance
ity σ ity σ ity σ ture (K) (mg) loss (%)
(K) ρ (Om m) ρ (Om m) ρ (Om m)
(S/sm) (S/sm) (S/sm)
I 298 6.9×108 1.4×10-11 II 8.4×108 1.1×10-11 III 10.9×108 0.9×10-11 293 0 −
303 6×108 1.6×10-11 7.9×108 13×10-11 9.8×108 1.0×10-11 313 0.4 3.63
308 6×108 1.6×10-11 7.4×108 1.4×10-11 9.8×108 1.0×10-11 333 1.0 9.09
313 5.6×108 1.7×10-11 6.9×108 1.4×10-11 9.6×108 1.1×10-11 353 1.5 13.63
318 5.6×108 1.7×10-11 6.5×108 1.5×10-11 9.1×108 1.1×10-11 373 2.0 18.18
323 5.2×108 1.9×10-11 6.1×108 1.6×10-11 8.7×108 1.2×10-11 393 3.4 30.9
328 5.2×108 1.9×10-11 5.9×108 1.7×10-11 8.3×108 1.2×10-11 413 4.5 40.9
333 4.8×108 2.1×10-11 5.7×108 1.8×10-11 7.9×108 1.3×10-11 433 5.0 45.0
338 4.6×108 2.2×10-11 5.3×108 1.9×10-11 7.6×108 1.3×10-11 453 5.4 45.09
343 4.2×108 2.4×10-11 4.9×108 2×10-11 7.1×108 1.4×10-11 473 5.8 52.72
348 3.8×108 2.6×10-11 4.6×108 2.2×10-11 6.5×108 1.5×10-11 493 6.0 54.54
353 3.8×108 2.6×10-11 4.1×108 2.4×10-11 6.2×108 1.6×10-11 513 6.4 58.11
358 3.2×108 3.1×10-11 3.8×108 2.6×10-11 5.4×108 1.9×10-11 533 6.6 60.0
363 2.8×108 3.6×10-11 3.8×108 2.6×10-11 4.7×108 2.1×10-11 553 7.4 62.27
368 2.4×108 4.2×10-11 3.5×108 2.9×10-11 4.1×108 2.4×10-11 573 8.5 77.27
593 10.3 93.63
613 10.8 98.18
 As it is obvious from Table 3 and Table 5, there is a direct dependence be-
tween the electrical conductance and the corrosion protection effect of the conser-
vative liquid; the higher electrical conductance, the greater corrosion protection
effect.
The experiment has been carried out according to the current standards in the
chamber called «CORROSİONBOX-1000E», which is considered as a modern
technological device. The process has been carried out in two phases: condensa-
tion and atmospheric phase.
The experiments were carried out with DC01 (CR4) carbon steel specimens
(ISO 3574). The test sample size was 150×100×1 mm. The mainly chemical com-
position (wt.%) of the carbon steel is given in Table 4.

Table 4. Chemical composition of the carbon steel

Element C Si Mn Ni S P Cr Al Cu Fe
Content (wt.%) 0.07 0.01 0.2–0.35 0.06 0.025 0.02 0.03 0.02–0.07 0.06 balance

The carbon steel plates were prepared, degreased and cleaned with deionized
water and alcohol. Electronic appliances have been used in order to adjust the
standard parameters for obtaining sustainable trials in the experimental chamber.
For the condensation phase, these parameters are the temperature of the chamber
and the duration of the trial, for the environmental phase, these are the tempera-
ture of the moisturizing agent and the chamber and the duration of the trial. The
duration of the trial was within the interval of 1 minute – 9999 hours and the
temperature of the chamber was 20 – 50°C for the condensation phase, whereas
the temperature of the moisturizing agent was 20 – 80°C and the remaining pa-
rameters were the same for the environmental phase.

RESULTS AND DISCUSSION

As it can be clearly seen from the Table 5, metal sheets were protected 31 and 56
days by using T-30 turbine oil and liquid rubber respectively. However, these indi-
ces were higher when inhibitor was used. When 7 % concentration of the inhibitor
(Sample I) was used, in the condensation phase, the protection of the metal sheets
from the corrosion lasted 312 days, however, in environmental phase, it was 371
days. In 10 % concentration, it was 348 and 415 days, respectively. At the same
time, the other tested conservation liquids, which were prepared by the composi-
tion of nitrocompound and amidoamines, which were synthesised by the reaction
of NPA and PEPA showed high results.
The dependence graph of the trial results of composition type conservation
liquids on the concentration of the inhibitor is shown below in Fig. 3.
257
Table 5. The trial results of the conservation liquids/lubricants

The duration of corrosion

The amount of the, protection, days
No Samples
inhibitor in sample, % condensation environmental
phase phase
1 Liquid rubber + T-30 oil 10 31 56
2 I +Т-30 oil 7 312 371
3 I +Т-30 oil 10 348 415
4 II+Т-30 oil 7 232 298
5 II+Т-30 oil 10 251 332
6 III+Т-30 oil 7 220 285
7 III+Т-30 oil 10 242 304
8 IV+Т-30 oil 7 237 296
9 IV+Т-30 oil 10 261 327
10 V+Т-30 oil 7 213 276
11 V+Т-30 oil 10 247 326
MWF 90%+ paraffin 10%
12 I+ paraffin 10 376 453
13 II+paraffin 10 361 433
14 III + paraffin 10 271 332
15 IV + paraffin 10 352 398
1 V + paraffin 10 324 372

Fig. 3. The graphical illustration

of the trial results of the conserva-
tion liquids

As it is clear from the figure, the highest result was obtained from the con-
servation liquid, which was synthesised by the composition of amidoamine with
NPA and PEPA with a mole ratio of 2:1 (curve I). The long lasting influence of the
aggressive environment on the metallic surface degrades the protective layer, as a
consequence, the coating loses its function at the certain level of the experience.

258
 As it is obvious from the Table 5, the lubricant, which is produced when
10% of technical paraffin is added to the MWF (Sample-I), which has the highest
efficiency in ‘corrosionbox’ protects metal plates for 376 and 453 days in conden-
sation and environmental phase, respectively. At the same time, the lubricants,
which are prepared by other metalworking fluids show high anti – corrosion effect
during the trial.

Scanning Electron Microscopy Analysis (SEM). Scanning Electron Microscope

(SEM: S-3400N HITACHI) morphologies of the steel plates in the corrosion box
in the absence and presence of MWF are shown in Fig. 4 (a–d) respectively.
Figure 4a shows the clean surface of steel sample before immersing in MWF. This
figure reveals the homogeneity of the surface. Figure 4b shows the general ap-
pearance of mild steel without inhibitor (only T-30 oil). It can be seen from the
figure that the surface of steel plates was extremely damaged in the absence of the
inhibitor. Figures 4c and d reflect the SEM morphology of the steel specimen at
lower concentration (5%) and higher concentration (10%) of the MWF. From the

Fig. 4a. The clean surface of steel sample before Fig. 4b. The general appearance of mild steel
immersing in MWF without inhibitor (only T-30 oil)

Fig. 4c. The SEM morphology of the steel spec- Fig. 4d. The SEM morphology of the steel
imen at lower concentration (5%) of the MWF specimen at higher concentration (10%) of the
MWF

259
figures it is clear that at low concentration (5%) of the MWF only few constituents
cover the surface, which are not enough to afford a protective layer and hence
dissolution of mild steel is observed to some extent, whereas at higher concen-
tration (10%) the constituents present are large enough to form a protective layer
regarding the dissolution of steel plates.

CONCLUSIONS

As a result of the experiments, it was revealed that when the synthesized amido-
amines and nitro compounds are applied as MWF and lubricants in the form of
composition, the protection effect of metal plates is higher (415, 453 and etc.). It
is explained that the compositions, which are produced by amidoamines and ni-
tro compounds create synergistic effect, which makes them to chemisorb on the
metal surface. On the other hand, these compounds are stronger ligands than the
water and that is why they can substitute water molecules from the surface of the
metal and create strong protection layer.
The components, which have been used for producing MWF are cost effec-
tive and environmentally – friendly, on the other hand, they have simple manu-
facturing technology and rich feedstock. T-30 oil, which is used as a medium,
additives and liquid rubber, which are used as inhibitors are produced on the basis
of the local feedstock. The results of the table of the experimental trials show that
the metalworking fluids and lubricants can be industrially applied as an effective
protection for processing and shipment of metal based products.

ACKNOWLEDGMENT

The authors are grateful for financial support of Research Institute of Petrochem-
ical Processes named after Yu. G. Mamedaliyev, Baku.

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